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研究生:李庭音
研究生(外文):Ting-Yin Lee
論文名稱:含三維結構五苯荑骨架之聚苯胺電極材料製備與作為超級電容器的應用
論文名稱(外文):Fabrication of the Three-dimensional Pentiptycene-incorporated Polyanilines for High Performance Supercapacitor Electrodes
指導教授:楊吉水
指導教授(外文):Jye-Shane Yang
口試日期:2017-07-14
學位類別:碩士
校院名稱:國立臺灣大學
系所名稱:化學研究所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2017
畢業學年度:105
語文別:中文
論文頁數:173
中文關鍵詞:五苯荑聚苯胺超級電容器電化學循環穩定性
外文關鍵詞:pentiptycenepolyanilinesupercapacitorelectrochemistrycycling stability
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超級電容器除了擁有高於電池的功率密度及穩定性,相較於傳統電容器,能量密度大幅提升,因此成為近幾年最有潛力的新興儲能裝置。其中,聚苯胺具有合成簡易、對環境污染較少、成本價格低廉及較高的理論電容儲存量等特性,最常被用來作為電容器電極材料;然而,聚苯胺在連續的充放電過程中,薄膜體積膨脹 / 收縮的改變則破壞本身的結構,使電容量嚴重衰退,進而影響後續的應用。為了克服穩定度不佳的問題,我們預測五苯荑分子H形剛硬結構有助於高分子鏈的嵌入,並以「夾子」形式穩固聚苯胺鏈,使鏈彼此有良好的堆疊排列,形成有效的交聯網絡,進而提升電容量與循環穩定性等電化學表現。為了引入三維立體剛硬結構的五苯荑分子至聚苯胺骨架,我們分別以DP、MA、DA和TA為起始物與苯胺進行共聚合反應,以探討起始物官能基如何影響共聚反應之聚合物DP-p、MA-p、DA-p和TA-p的結構與性質。
結果顯示MA、DA及TA分子有效作為模板並參與聚合反應,由電子顯微鏡觀測其聚合物表面形態為球形堆疊結構,然而DP-p則相似於PANI顆粒團狀結構。於電化學表現上,球形堆疊之TA-p電容儲存量高達410 F / g,千圈穩定度為91 %;DA-p與MA-p電容量分別為330 F / g和250 F / g,穩定度亦提升至87 %左右,皆高於兩者顆粒團狀之DP-p與PANI聚合物,其電容量僅約220 F / g且電容保存率剩70 %左右。此表示五苯荑分子確能發揮「夾子」功用,使聚苯胺鏈間進行有效排列,亦能穩固聚苯胺鏈抑制其在長時間測試中骨架的裂解,進一步提升材料整體的電化學性質。
比較這四種系列的五苯荑對聚苯胺分子鏈在空間上的分佈與互相堆疊的影響,研究形成的聚合物在電化學上的表現,有助於日後超級電容器電極材料的改良,在儲能裝置上達到更有效的利用。
Supercapacitors, used as energy storage devices, have the feature of higher power density and durability than batteries and higher energy density than conventional dielectric capacitors. Polyaniline is one of the most useful conducting polymers as the supercapacitor electrode materials due to its high theoretical specific capacitance. During the charge / discharge processes, however, the PANI-based electrodes have poor long-term stability because of swelling / shrinkage.
To improve the stability, we reasoned that the rigid H-shaped pentiptycene scaffold will act as a “clip” for fixing polyaniline chains in plane, which promotes the formation of internal interlocking structure. Therefore, we have prepared a series of pentiptycene derivates, DP, MA, DA and TA to react with aniline to form pentiptycene-incorporated polyanilines, and then explored the relationship between the starting materials and the properties for the polymers.
Our results indicate that MA, DA and TA are good materials for the chemical oxidative polymerization. The polymer MA-p, DA-p and TA-p display spherical morphology, but DP-p is similar to the parent polyaniline (PANI), which shows a granular structure. Regarding the electrochemical performance, TA-p shows the best capacitance, 410 F / g, and retains 91 % capacity after 1000 charge-discharge cycles;MA-p and DA-p also indicate higher capacitance, 330 F / g and 250 F / g, respectively, than DP-p and PANI, and show about 87 % capacitance retention during long-term process.
The rigid H-shaped pentiptycene effect on the enhanced capacitive performance of polyanilines might stimulate the future modification and application of model polyanilines as the electrode materials of supercapacitors.
謝誌......................................................i
摘要....................................................iii
Abstract.................................................iv
目錄......................................................v
圖目錄...................................................ix
表目錄..................................................xiv
附圖目錄..................................................xv
第一章 緒論................................................1
1-1 能源儲存...............................................1
1-2 超級電容器.............................................3
1-2-1 超級電容器原理.......................................3
1-2-2 超級電容種類.........................................4
1-2-3 超級電容器電極材料分析................................8
1-3 聚苯胺................................................9
1-3-1 聚苯胺簡介與導電原理..................................9
1-3-2 聚苯胺之聚合反應機制.................................13
1-3-3 聚苯胺的奈米結構....................................16
1-3-4 聚苯胺的合成方式....................................17
1-3-5 寡聚物添加對聚苯胺奈米結構的影響......................19
1-4 聚苯胺在超級電容上的應用...............................21
1-4-1 聚苯胺應用於超級電容器的限制.........................21
1-4-2 聚苯胺超級電容的改善方針.............................22
1-4-3 混合式超級電容器的應用...............................23
1-4-4 共軛導電高分子之奈米結構和表面性質的改善..............25
1-4-5 聚苯胺高分子鏈的本質改變.............................27
1-5 超級電容器的介面化學分析...............................28
1-5-1 介面化學分析........................................28
1-5-2 掃描式電子顯微鏡....................................28
1-5-3 穿透式電子顯微鏡....................................29
1-5-4 BET比表面積及孔徑分析儀.............................30
1-6 超級電容器的電化學分析.................................34
1-6-1 電化學分析介紹......................................34
1-6-2 循環伏安法..........................................34
1-6-3 恆電流充放電法......................................35
1-6-4 電化學阻抗頻譜法....................................36
1-6-5 四點探針之電阻測量..................................39
1-7 含五苯荑分子之共軛聚合物...............................42
1-7-1 苯荑分子及其衍生物..................................42
1-7-2 五苯荑分子合成與官能化發展...........................43
1-7-3 苯荑分子於共軛高分子之應用...........................44
1-8 研究動機..............................................49
第二章 結果與討論.........................................51
2-1 單體化合物之合成及電化學特性分析........................51
2-1-1 合成策略分析........................................51
2-1-2 五苯荑分子及其衍生物之合成...........................52
2-1-3 含五苯荑單體分子之電化學分析.........................55
2-2 含五苯荑骨架之聚苯胺的聚合及性質鑑定....................57
2-2-1 含五苯荑骨架之聚苯胺的聚合反應........................57
2-2-2 含五苯荑骨架之聚苯胺的結構鑑定........................61
2-2-3 含五苯荑骨架之聚苯胺的性質量測........................68
2-3 含五苯荑骨架之聚苯胺奈米結構與表面形態..................71
2-3-1 含五苯荑骨架之聚苯胺的SEM 掃描圖.....................71
2-3-2 含五苯荑骨架之聚苯胺的TEM 掃描圖.....................75
2-3-3 含五苯荑骨架之聚苯胺的奈米結構分析....................79
2-4 含五苯荑骨架之聚苯胺的表面分析..........................80
2-4-1含五苯荑骨架之聚苯胺的氮氣吸附-脫附等溫曲線與孔徑尺寸分佈 .........................................................80
2-5 含五苯荑骨架之聚苯胺的電化學分析........................82
2-5-1 含五苯荑骨架之聚苯胺的循環伏安法分析..................82
2-5-2 含五苯荑骨架之聚苯胺的恆電流充放電分析................86
2-5-3 含五苯荑骨架之聚苯胺的電化學阻抗光譜分析..............89
2-5-4 含五苯荑骨架之聚苯胺的循環穩定度分析..................91
2-5-5 含五苯荑骨架之聚苯胺的導電度量測......................93
2-5-6 含五苯荑骨架之聚苯胺的電化學分析比較..................95
第三章 結論...............................................96
第四章 實驗部分...........................................97
4-1實驗藥品與溶劑.........................................97
4-2 實驗儀器.............................................101
4-2-1 化合物/聚合物結構之鑑定.............................101
4-2-2 純化系統...........................................103
4-2-3 聚合物表面化學與熱穩定性質之量測.....................103
4-2-4 聚合物超級電容器電極材料之電化學性質量測.............105
4-3 實驗步驟............................................107
4-3-2 五苯荑及其衍生化合物之合成..........................107
4-3-2 聚苯胺及含五苯荑骨架聚合物之合成.....................119
參考資料.................................................123
附圖....................................................132
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